Deuterated chloroform (CDCl3) is a common solvent used in nuclear magnetic resonance (NMR) spectroscopy measurements. Industrially, CDCl3 is typically produced through two methods—a reaction of deuterated acetone or ethanol and an alkali metal hypochlorite, or a reaction of chloral hydrate with sodium deuteroxide. Previously reported laboratory scale synthesis of CDCl3 includes reacting chloroform (CHCl3) with deuterium oxide (D2O) and sodium metal or sodium peroxide, or catalytic NaOD. However, the use of sodium metal or sodium peroxide poses a safety hazard on an industrial setting, while the use of catalytic NaOD uses a large excess of deuterium oxide with only a moderate product yield. Another method was to react hexachloro-2-propanone (hexachloroacetone) with pyridine and deuterium oxide, however side products are formed which require distillation to purify the deuterated chloroform. In addition, the side production formation requires the replenishment of pyridine adding to the cost and inefficiency of the process.